US20110198358A1 - Article with a ceramic coating and method for producing such an article using a laser - Google Patents

Article with a ceramic coating and method for producing such an article using a laser Download PDF

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US20110198358A1
US20110198358A1 US12/997,574 US99757409A US2011198358A1 US 20110198358 A1 US20110198358 A1 US 20110198358A1 US 99757409 A US99757409 A US 99757409A US 2011198358 A1 US2011198358 A1 US 2011198358A1
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Prior art keywords
ceramic
coating
layer
substrate
metallic
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US12/997,574
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Fabrice Parent
Laurent Voisin
Jean-Luc Perillon
Arnaud Hory
Quentin Joly
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SEB SA
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SEB SA
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Publication of US20110198358A1 publication Critical patent/US20110198358A1/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • A—HUMAN NECESSITIES
    • A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
    • A47J—KITCHEN EQUIPMENT; COFFEE MILLS; SPICE MILLS; APPARATUS FOR MAKING BEVERAGES
    • A47J36/00—Parts, details or accessories of cooking-vessels
    • A47J36/02—Selection of specific materials, e.g. heavy bottoms with copper inlay or with insulating inlay
    • A—HUMAN NECESSITIES
    • A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
    • A47J—KITCHEN EQUIPMENT; COFFEE MILLS; SPICE MILLS; APPARATUS FOR MAKING BEVERAGES
    • A47J37/00—Baking; Roasting; Grilling; Frying
    • A47J37/10—Frying pans, e.g. frying pans with integrated lids or basting devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
    • B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
    • B05D5/086—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers having an anchoring layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
    • Y10T428/12542—More than one such component
    • Y10T428/12549—Adjacent to each other
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
    • Y10T428/12556—Organic component
    • Y10T428/12569—Synthetic resin
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/1266—O, S, or organic compound in metal component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12736—Al-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12951—Fe-base component
    • Y10T428/12972—Containing 0.01-1.7% carbon [i.e., steel]
    • Y10T428/12979—Containing more than 10% nonferrous elements [e.g., high alloy, stainless]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/21—Circular sheet or circular blank
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
    • Y10T428/24851—Intermediate layer is discontinuous or differential
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
    • Y10T428/24917—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.] including metal layer

Definitions

  • the present invention relates generally to an article comprising a metal substrate comprising two principal faces and at least one ceramic coating covering at least one of these faces, as well as a manufacturing process for such an article in which the ceramic coating is fritted by laser beam.
  • ceramic coatings are applied in the form of an aqueous suspension or slip containing a refractory powder, then fitted by heat treatment (by firing in an oven, for example) during which the grains of refractory powder are fused together by the effect of heat, which results in the consolidation of the coating.
  • sintering is generally achieved by firing during which the fusion of the enamel powder occurs, followed by cooling during which the vitrification of the enamel takes place.
  • the enamel fit must be applied onto a substrate that is able to withstand the fusion temperature of the enamel (or more precisely its softening temperature).
  • sintering carried out by an oven-firing type thermal route does not allow the creation of a ceramic coating, particularly of the enamel type, on a substrate whose constitutive material has a fusion temperature below the softening point of the ceramic coating, because that would necessarily lead to the melting of the substrate.
  • U.S. Pat. No. 3,663,793 describes a process for forming a mark or a design on the surface of an article such as a lamp case made of soda-lime glass.
  • This process comprises a step in which at least part of the surface is coated with a pigmented vitreous frit containing lead oxide in particular and occurring in the form of a slip or aqueous suspension, then an air-drying step to form a powdery layer.
  • the case thus coated is subjected simultaneously to the action of a burner flame and that of a laser beam.
  • the burner flame's action allows firing of the powdery layer at a temperature of the order of 700° C., during which it is transformed into a white enamel or glaze type coating.
  • the white enamel (or glaze) thus formed constitutes a durable and tough coating which will not fracture when it is subjected to laser radiation. If the burner flame is adjusted to be reducing, the lead oxide in the glaze is transformed into lead under the effect of the laser beam.
  • Japanese patent application JP 2 279 574 a process for decorating the surface of a wall which may be of brick, of cement, of steel or of aluminium.
  • This process comprises a step in which a vitreous material is flame-sprayed onto the surface of a wall to form there a layer of the vitreous coating, followed by a step in which certain areas of the surface thus coated are irradiated with a laser beam, to form a film of enamel over the vitreous coating.
  • the enamel layer on the vitreous coating is in fact made up of the coating previously vitrified during flame spraying, on the surface of which the effect of the laser is manifested by the transformation of certain compounds of the coating, thus creating in the irradiated areas a decorative layer of a superficially different nature from the vitreous coating.
  • the laser in the process of JP 2 279 574 is not used to frit the vitreous composition, but only to create the decorative design.
  • a laser decoration, marking and engraving process for objects with enamelled surfaces is known from French patent application FR 2 575 422.
  • This process comprises a prior step of mixing opacifiers into an enamel which dissociate locally and by optical effect (of the oxides of titanium, of tin, of cerium or of antimony, for example), then a step of optical action on the enamel using a laser beam, for example a CO 2 laser or a YAG laser.
  • International application WO 99/16625 describes a method of marking by thermal activation of a substrate, in particular of stainless steel or of aluminium. This method is based on the laser irradiation of a uniform and continuous layer of a marking material suited to the substrate (particularly of the glass or enamel frit type), this marking material containing a concentrate that absorbs the energy of a laser beam to create a bond to the substrate.
  • the glass or enamel frit occurs in the form of a slip that is oily rather than aqueous, and which therefore has a tendency to spread. It is therefore not possible to form, before sintering, a discontinuous coating.
  • the sintering of such a slip has a tendency to produce soot, the presence of which on the surface of the substrate could interfere with the adhesion of the coating to be formed.
  • the portion of the marking material that is irradiated by the laser beam is also continuous, which has the consequence that the substrate may not undergo any deformation after irradiation.
  • the enamel or glass frit is formulated in the form of an oily slip, there is a consequent coking of the oil during sintering. This coking of the oil, however, consumes a considerable part of the energy delivered by the laser, which is greater than that needed for evaporating water. The energy efficiency of the laser is thereby reduced.
  • the present invention addresses all or part of the above described disadvantages, by forming a discontinuous ceramic or metallic coating fritted by the laser route, occurring in the form of a superficial dispersion of solidified drops of ceramic or metallic material on a substrate, with a lower, even near-zero density in the parts of the substrate that are intended to undergo deformation, particularly of the stamping type.
  • Sintering by the laser route of such a coating makes it possible, on the one hand, to escape the substrate constraint, which can then be constituted of a material with a low melting point, while the coating can be a material with a high melting or softening point; and on the other hand to deposit such a coating without incurring an excessive expenditure of energy.
  • embodiments of the present invention propose an article comprising a metal substrate comprising two opposed faces, and a ceramic or metallic coating covering at least one of the faces of the substrate, the ceramic or metallic coating having a softening point that is higher than the melting temperature of the substrate, and comprising at least one component that absorbs laser radiation with a wavelength of the order of 1 ⁇ m, constituting at least 1% of the weight of the coating,
  • the ceramic or metallic coating is a discontinuous layer having a surface roughness Ra of between 2 ⁇ m and 10 ⁇ m and a thickness of between 5 and 30 ⁇ m.
  • discontinuous layer means a superficial dispersion of solidified drops of the ceramic or metallic material, these drops having a mean size of between 1 and 40 ⁇ m, and being distributed homogeneously on the surface of the coated face, with a coverage of that surface of between 30 and 80%.
  • the term superficial dispersion of solidified drops of ceramic or metallic material means a layer of ceramic or metallic material occurring in a divided state on a substrate (in this case that of a cookware article), such that the roughness of this layer is created by the solidified drops of ceramic or metallic material.
  • coverage means the ratio, expressed in percent, of the substrate surface area actually covered by the superficial dispersion of solidified drops to the total substrate area that can be covered.
  • ceramic material means any inorganic, essentially non-metallic material.
  • non-metallic means that the material has an inorganic lattice in which there may be very small quantities of metallic elements such as aluminium, iron, titanium, lithium, sodium, potassium, calcium.
  • Ceramic materials being refractory materials having heterogeneous compositions and structures, they do not have uniform melting points. For such materials, the refractoriness is generally defined by the softening point.
  • softening point or temperature of a refractory material means the temperature at which the material softens or begins to soften and attains a certain consistency under standardized conditions.
  • metallic material means any metal or metal alloy capable of absorbing laser radiation at a wavelength of the order of 1 ⁇ m.
  • stainless steels food grade, and preferably 304 and 309 stainless steels
  • titanium and nickel can be mentioned in particular.
  • the coating comprises a component that absorbs the radiation emitted by the laser operating at a given wavelength.
  • the term absorbing component is taken to mean a substance used to absorb the energy of a given type of radiation.
  • component absorbing laser radiation at a given wavelength means a substance used to absorb the energy of laser radiation emitted by a laser emitting at that wavelength.
  • a laser operating at a wavelength of the order of 1 ⁇ m can be used to advantage, as for example a line laser emitting a wavelength of 980 nm, or a fiber laser emitting at a wavelength of 1,064 nm.
  • an absorbing component selected from among the stainless steels (preferably those approved within the scope of food preparation use), the metal oxides, particularly among the oxides of aluminium (Al 2 O 3 ), of titanium (TiO 2 ), the iron oxides, the mixed oxides of copper, iron and manganese, silicon carbide, tungsten carbide and graphite.
  • a metallic coating as that term is used in the present invention, it is by nature made up of a material that absorbs laser radiation at a wavelength of the order of 1 ⁇ m, and it is therefore not necessary to add an additional component that absorbs laser radiation to the aqueous metal powder suspension that is applied to the support for the purpose of forming the coating.
  • a ceramic coating made up for example of alumina or titania which are also materials that absorb laser radiation at a wavelength of 1 ⁇ m.
  • the coating is made of an inorganic material obtained by fusing an enamel frit for instance, it is necessary to add at least 1% by weight, referred to the weight of the fit, of at least one component that absorbs laser radiation at a wavelength of the order of 1 ⁇ m to the aqueous suspension of enamel frit (or slip) that is applied to the substrate.
  • an enamel frit comprises alumina in its composition (which is that obtained after transition to the molten state)
  • the aluminium that enters into the composition of the enamel fit is no longer in the form Al 2 O 3 : it is included in an inorganic lattice, that is to say connected to other elements besides aluminium (Al) and oxygen (O).
  • organic dyes organic absorbers, as for example the organic borate dyes developed by the Exciton company
  • mineral pigments such as the oxides of cobalt, of chromium, and in particular mineral pigments based on CoCrFeNi, ZrSiCoNi, CoAl.
  • the ceramic coating is a coating that comprises enamel, whose composition is suited to the nature of the substrate, in particular an “aluminium enamel,” a “glass enamel,” a “sheet steel enamel” (preferably stainless steel) or a “ceramics enamel”.
  • aluminium enamel means an enamel with a low softening point (below 600° C.).
  • glass enamel means an enamel with a softening point between 600 and 650° C.
  • sheet steel enamel (preferably stainless) means an enamel with a softening point near 800° C.
  • ceramics enamel means an enamel with a very high softening point (higher than 900° C. in particular).
  • the parameters of the laser must be suited to the nature of the enamel used.
  • the power of the laser beam, the laser beam's scan rate, the impulse time, the frame period are parameters to be adjusted to match the enamel and the quantity of radiation-absorbing components present in the composition of the enamel; less energy is required for enamels with low fusion points than for enamels with high fusion points.
  • (laser power/scan rate) pairs allowing sintering to be carried out, (4 to 5 kW, 10 to 15 m/s), (200 W, 2 m/s) and (50 W, 400 to 500 m/s) are recommended.
  • the substrate is made of aluminium or aluminium alloy.
  • a “sheet steel enamel” whose composition typically contains:
  • fluxing component means any substance present within the enamel composition which, even in minimal quantity, lowers the softening point of the ceramic material.
  • alkalis and alkaline earths or more particularly sodium oxide, potassium oxide, boron oxide, bismuth oxide and vanadium oxide are recommended.
  • enamellable low-alloy aluminium alloys and aluminium casting alloys are recommended.
  • enamellable low-alloy aluminium alloys are:
  • aluminium casting alloys suitable for use in making the substrate of the article according to embodiments of the invention it is possible to use any kind of aluminium-silicon AS alloy, and particularly the aluminium-silicon alloys which are customarily produced in connection with enamelling because they have a fusion temperature close to or even below the softening point of the enamels. More particularly recommended are the AS7 to AS12 type aluminium-silicon AS alloys, that is AS alloys containing from 7 to 12% silicon in accordance with former French standard NF AS 02-004.
  • the substrate is made of stainless steel.
  • the enamel coating can be a conventional enamel such as a “sheet steel enamel,” preferably stainless, with the weighbatching composition:
  • Oxides of barium, cobalt, nickel, copper, titanium, manganese ⁇ 3% for each compound.
  • the article may also comprise, besides the enamel coating covering at least one of the principal faces of the substrate, a non-stick coating including at least one layer including at least one fluorocarbon resin, alone or mixed with a thermally stable bonding resin tolerating at least 200° C., this bonding resin forming a continuous fritted lattice after sintering.
  • fluorocarbon resins usable in the non-stick coating according to the invention polytetrafluoroethylene (PTFE), tetrafluoroethylene-perfluoropropylvinylether copolymer, tetrafluoroethylene-hexafluoropropylene copolymer (FEP), and their mixtures (particularly a mixture of PTFE and PFA) are recommended.
  • PTFE polytetrafluoroethylene
  • FEP tetrafluoroethylene-hexafluoropropylene copolymer
  • PFA tetrafluoroethylene-hexafluoropropylene copolymer
  • the polyamide-imides (PAI), the polyetherimides (PEI), the polyimides (PI), the polyetherketones (PEK), the polyether-etherketones (PEEK), the polyethersulfones (PES) and the polyphenylene sulfides (PPS) and their combinations are recommended.
  • the non-stick coating covering the hard enamel base can comprise a layer of bonding primer and at least one finish layer, at least one of the finish layers defining a surface layer, the primer layer and the finish layer(s) each comprising at least one fritted fluorocarbon resin, alone or in admixture with a thermally stable bonding resin tolerating at least 200° C., which form(s) a continuous fritted lattice of fluorocarbon resin, and of bonding resin if applicable.
  • the primer layer can also comprise mineral or organic fillers and/or pigments.
  • colloidal silica As fillers usable in the primer composition of the article according to the invention, colloidal silica, mica flakes coated with TiO 2 , alumina, corundum, quartz and their mixtures can be mentioned in particular.
  • the non-stick coating can comprise, particularly in the primer, a component that absorbs laser radiation at a wavelength of 10.6 ⁇ m.
  • metal oxides particularly iron oxides
  • the sintering of such a coating can be advantageously carried out by the laser route even if this coating does not comprise a component that absorbs laser radiation at a wavelength of 10.6 ⁇ m.
  • the laser beam passes through the non-stick coating and is absorbed by the underlying ceramic coating, which heats it by thermal conduction.
  • the non-stick coating comprise fillers facilitating thermal conduction within the non-stick coating, and more particularly through the bonding primer.
  • fillers facilitating thermal conduction within the non-stick coating, and more particularly through the bonding primer.
  • flat disc means a solid round metal part, commercially flat, cut from a sheet or a strip.
  • cookware articles such as pots and pans, woks and frying pans, crepe makers, grills, moulds and plates for pastry-making, barbecue grills and griddles are particularly mentioned.
  • process sintering includes:
  • the ceramic or metal powder is present in the ceramic or metallic composition at the rate of 45% to 75% by weight of the total weight of said composition.
  • Such a process has the advantage of sharply limiting the energy consumption that is usually needed for sintering a ceramic coating, particularly of the enamel type, by reducing it by a factor of 100 with respect to sintering by a thermal route.
  • each drop of ceramic or metallic material is integral with sufficiently strong adhesion to the substrate to allow it to undergo slight deformations without detaching the discontinuous layer from it.
  • the ceramic or metallic composition sintering step is carried out by a laser beam irradiating in a continuous scan (in the form of lines with a definite thickness and interval between lines) at least a part of the face coated with the ceramic composition.
  • the ceramic composition sintering step is carried out by a laser beam irradiating in a discontinuous scan (in the form of spots having a definite diameter and interval) at least a part of the face coated with the ceramic composition.
  • FIG. 1 is a schematic section view of a cookware article conforming to the invention according to a first embodiment
  • FIG. 2 is a schematic section view of a cookware article conforming to the invention according to a second embodiment
  • FIG. 3 is a schematic section view of a cookware article conforming to the invention according to a third embodiment.
  • FIGS. 1 to 3 Identical components shown on FIGS. 1 to 3 are identified by identical reference numbers.
  • FIGS. 1 to 3 depict, by way of example of a cookware article according to embodiments of the invention, a pan 1 comprising a metal substrate 2 occurring in the form of a hollow shell provided with a handle 5 , the shell comprising a bottom 1 and a side wall rising from bottom 1 .
  • Substrate 2 comprises an inner face 21 which is the face oriented toward the food to be accommodated in pan 1 , and an outer face 22 which is intended to be arranged toward an outside heat source.
  • Inner face 21 is successively coated, beginning at substrate 2 , with a ceramic or metallic coating 3 and with a non-stick coating 4 which comprises successively, beginning at the hard base 3 , a bonding primer layer 41 and two finish layers 42 , 43 .
  • Coating 3 thus constitutes a hard base for the non-stick coating 4 that covers it.
  • the ceramic or metallic coating 3 covering inner face 21 of substrate 2 is a discontinuous layer, having a surface roughness Ra of between 2 ⁇ m and 10 ⁇ m and a thickness of between 5 and 30 ⁇ m, preferably between 5 ⁇ m and 15 ⁇ m.
  • This discontinuous layer 3 is in fact made up of a superficial dispersion of drops of ceramic or metallic material which are solidified and have a mean size of between 1 ⁇ m and 40 ⁇ m.
  • the solidified drops are homogeneously distributed over the entire surface of inner face 21 , with an inner face 21 coverage of between 30 and 80%.
  • the superficial dispersion of solidified drops 31 , covering inner face 21 of substrate 2 to make up the ceramic coating 3 is not uniform.
  • the enamel drop density is maximal in the central part of the bottom 12 of pan 1 , and decreases toward the side wall 11 .
  • a third variation of a cookware article according to an embodiment of the invention also has a superficial dispersion of drops of ceramic or metallic material 31 , which are solidified and cover the inner face 21 of substrate 2 .
  • This dispersion is also not uniform.
  • the density of solidified drops 31 is nil in the joining zone 13 between the bottom 11 and the side wall 12 of the pan (which corresponds to the part of the article during forming, particularly by stamping), and the density of solidified drops 31 is maximal in the central part of bottom 12 and the side wall, which are the parts of the pan that undergo no deformation during forming, particularly by stamping.
  • the drops of ceramic or metallic material 31 which are dispersed on the surface of inner face 2 , are embedded in the primer layer 41 of non-stick coating 4 , so as to allow bonding of the primer layer, so that increased mechanical reinforcement of non-stick coating 4 is obtained, particularly in terms of hardness and adhesion to the underlying hard base 3 .
  • the particles of fitted fluorocarbon resin and the fillers in primer layer 41 by penetrating between the solidified drops 31 of ceramic or metallic material deposited on the surface of inner face 21 , strengthen the adhesion of the primer layer 41 to hard base 3 .
  • the mechanical reinforcement of non-stick coating 4 is increased both because of the fillers in primer layer 41 and because of the dispersion of solidified drops 31 of hard base 3 which play a role similar to that of a reinforcing filler in the interpenetration zone of the two layers 3 , 41 .
  • FIG. 3 shows that the outside face 22 of substrate 2 can be advantageously coated with an outside enamel coating 6 .
  • the thickness of this outside (or cover) enamel coating 6 is conventionally between 40 ⁇ m and 500 ⁇ m, particularly between 40 ⁇ m and 100 ⁇ m for an aluminium alloy substrate (low alloy or aluminium casting), between 200 ⁇ m and 500 ⁇ m for a cast iron substrate (meaning an alloy of iron and carbon with more than 21% carbon) and lastly between 100 ⁇ m and 200 ⁇ m for a stainless steel substrate.
  • the metal shell 2 used as a substrate is advantageously made of aluminium or aluminium alloy, as an aluminium casting (or of an aluminium casting alloy), of stainless steel, of cast iron (an alloy in the sense of the term's sign, to wit, an alloy with more than 21% carbon), or of copper.
  • substrate 2 has the final shape of a cookware article, with a concave inner face 21 intended to be set next to the food to be put the said article 1 , and a convex outer face 22 intended to be set next to a heat source.
  • the forming of the article is carried out before the deposition of any coating, whether internal or external.
  • the step of forming substrate 2 is carried out after the step of creating non-stick coating 4 on internal discontinuous hard base 3 .
  • a flat substrate is therefore employed, a disc for example, which will be stamped after the sintering step.
  • the step of applying the ceramic or metallic composition 3 a to at least one of the faces 21 of the substrate is preceded by a surface preparation step.
  • the application of the ceramic or metallic composition 3 a to inner face 21 is preceded by a surface preparation step which may vary according to the nature of the substrate:
  • aqueous composition 3 a comprises from 45% to 75% by weight of a ceramic or metallic powder, with at least one component absorbing laser radiation at a wavelength of the order of 1 ⁇ m, which makes up at least 1% referred to the total weight of the powder.
  • a ceramic or metallic composition ( 3 a ) usable in the process of the invention it is possible to use an aqueous slip of enamel fit, or an aqueous suspension of alumina, or of titanium dioxide, or even an aqueous suspension of stainless steel powder (preferably food grade), or a mixture of these various compounds.
  • the sintering step is carried out by laser radiation irradiating at least partially face(s) 21 , 22 coated with refractory composition 3 a , at a wavelength of the order of 1 ⁇ m.
  • the laser beam contributes the energy needed for sintering the irradiated portions coated with the refractory composition 3 a and creating the ceramic coating 3 .
  • a fiber laser of the YAG type operating at a power level of 50 Watts and emitting at a wavelength of 1,064 nm can be used, or a line laser operating at a power level of the order of 350 Watts and emitting at a wavelength of 980 nm.
  • the power of the laser (fiber or line) must be matched to the production rate, and could possibly exceed 50 W or 350 W.
  • the ceramic or metallic composition 3 a is applied so as to form a continuous non-sintered layer 3 and the sintering step is carried out by a laser beam irradiating in a discontinuous scan this non-fitted layer 3 .
  • the ceramic or metallic composition 3 a is applied so as to form a discontinuous non-fritted layer 3 and the sintering step is carried out by a laser beam irradiating in a discontinuous and/or continuous scan this non-fritted layer 3 .
  • Discontinuous scanning can for example be carried out by a 4,000 W fiber laser with an 800 ⁇ m spot, which automatically scans out a predefined grid representing a number of pixels (in dpi, or number of laser impact points) on the surface of the discs. This makes it possible to leave unfitted the parts that will be deformed during the forming of the substrate (particularly by stamping).
  • the aqueous suspension dispersion of ceramic or metallic powder can be applied to the inner face 21 of substrate 2 by pneumatic spraying under a spraying pressure greater than or equal to 4 bars, and the quantity of enamel deposited onto said inner face 21 is between 0.1 g/dm 2 and 3 g/dm 2 .
  • the non-stick coating 4 on enamel layer 3 is carried out by depositing at least one layer of fluorocarbon resin-based composition 4 a , then a sintering step to form a non-stick coating 4 occurring in the form of a continuous fritted lattice of fluorocarbon resin, regardless of the nature of the ceramic (particularly an aqueous suspension of alumina or titanium dioxide or an aqueous enamel fit slip) or metallic (particularly an aqueous suspension of stainless steel powder) composition.
  • non-stick coating 4 can be carried out either thermally in an oven, at a temperature of between 370° C. and 430° C., or with a CO 2 laser whose wavelength is 10.6 ⁇ m. This wavelength allows a more homogeneous heat treatment to be obtained.
  • Coating compositions these are aqueous suspensions of enamel fit or of alumina, titanium dioxide or steel powder, whose characteristics are given below:
  • Frit F1 of “aluminium enamel” with weighbatching composition is
  • Al 2 O 3 less than 1%
  • Frit FC1 of “aluminium enamel” with weighbatching composition
  • Al 2 O 3 less than 1%
  • V 2 O 5 less than 10%.
  • Frit F2 of “sheet steel enamel” with weighbatching composition is
  • Oxides of barium, cobalt, nickel, copper, titanium, manganese ⁇ 3% for each compound.
  • Iron (III) oxide Fe 2 O 3
  • iron (II) oxide FeO
  • the abrasion resistance of the non-stick coating formed is evaluated by subjecting it to the action of a green SCOTCH BRITE ⁇ type abrasive pad.
  • the coating's abrasion resistance is quantitatively estimated by the number of passes with the pad needed to create the first scratch (exposing the metal of which the substrate is made).
  • the non-stick characteristic is measured according to the greater or lesser ease of cleaning off charred milk.
  • the rating scheme is as follows:
  • the adhesion of the fritted (or sintered) ceramic or metallic coating to the substrate is also evaluated.
  • a checkerboard test is done per ISO 2409 standard, followed by immersion of the article for 9 hours (three cycles of three hours in boiling water). Then the non-stick coating is inspected to see whether or not it shows detachment.
  • the rating scheme is as follows:
  • the value assigned is 100 minus the number of detached squares.
  • the procedure is as follows: the plate is subjected to the action of a hemispherical punch 20 mm in diameter, weighing 2 kg and falling 50 cm onto the back face. The coated face is inspected.
  • a coating composition according to the process of an embodiment of the invention is applied to one of the faces of the substrates.
  • the second face can either be processed the same way (that is by sintering by the laser route) or processed in the traditional manner (that is by firing in an oven at a temperature of the order of 560° C.).
  • Results of the abrasion resistance test show that after 20,000 “round trip” passages of an abrasive pad, the coating shows no scratches exposing the metal.
  • the non-stick characteristic evaluated by the burnt milk test gives a score of 50.
  • the hard base remains in the form of a powder deposit not adhering to the metal substrate.
  • the interior coating (inner face) does not show any visible fissures.
  • test results show that the first scratch (exposing the metal constituting the substrate) is visually observed (under 8 ⁇ optical magnification) only after 20,000 passes with the pad.
  • Adhesion measured by the checkerboard test after immersion is excellent: no squares are torn off.
  • the non-stick characteristic evaluated by the burnt milk test gives a grade of 100.
  • Test results are comparable to those obtained in Example 1, but with a much higher energy consumption.
  • the temperature variation ⁇ T 2 that the enamel frit undergoes is 2,500° C. ⁇ 20° C. (ambient temperature), that is a temperature variation of 2,420K,
  • the specific heat Cp 2 of the frit is 800 J/kg*K.
  • the energy consumption ⁇ Q 2 of sintering by the laser route is only 2,381 J, that is an energy consumption reduction of more than 98% (98.7% exactly) compared to oven firing at 560° C.
  • the energy consumption ratio ⁇ Q 1 / ⁇ Q 2 is 1.22%, which corresponds to a reduction of energy consumption of 98.7% when switching from oven firing at 560° C. to sintering by the laser route under the experimental conditions given earlier.
  • the laser's efficiency is of the order of 66% and the residual heating of the disc is slight (a few degrees), even with a continuous scan.
  • the abrasion test results show that after 20,000 “round trip” passes of an abrasive pad, the coating shows no scratches extending to the metal.
  • the non-stick characteristic evaluated by the burnt milk test gives a rating of 50.
  • the firing temperature is insufficient for hardening the hard base, which remains in powder form with no adhesion to the substrate.
  • firing at a higher temperature 650° C. in particular, which is a temperature allowing the hardening and sintering of the hard base, leads to fusion and deformation of the substrate.
  • Comparison of Examples 2 and C2 therefore shows that laser sintering makes it possible to gain access to basic formulations having fusion points higher than those of the substrate.
  • This interior coating does not show any visible fissures.
  • the adhesion measured by the checkerboard test after immersion is poor: several squares are torn out by virtue of the presence of non-adhering carbon particles resulting from combustion of the oil.
  • the interior coating (on the inner face) of the article thus obtained shows no visible fissures.

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  • Organic Chemistry (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Food Science & Technology (AREA)
  • Cookers (AREA)
  • Laminated Bodies (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Laser Beam Processing (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Making Paper Articles (AREA)
US12/997,574 2008-07-29 2009-07-24 Article with a ceramic coating and method for producing such an article using a laser Abandoned US20110198358A1 (en)

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FR0855221A FR2934591B1 (fr) 2008-07-29 2008-07-29 Article comprenant un revetement ceramique et procede de fabrication d'un tel article mettant en oeuvre un laser.
PCT/FR2009/051504 WO2010012944A2 (fr) 2008-07-29 2009-07-24 Article comprenant un revêtement céramique et procédé de fabrication d'un tel article mettant en oeuvre un laser.

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ATE540140T1 (de) 2012-01-15
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CN102083621A (zh) 2011-06-01
CN102083621B (zh) 2014-05-07
EP2307590A2 (de) 2011-04-13
EP2307590B1 (de) 2012-01-04
FR2934591B1 (fr) 2011-02-11
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ES2377282T3 (es) 2012-03-26
BRPI0910012B1 (pt) 2019-03-26

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